CN109588753B - Formula design method and application of tobacco leaf group of heating non-combustible cigarette - Google Patents
Formula design method and application of tobacco leaf group of heating non-combustible cigarette Download PDFInfo
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/08—Blending tobacco
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
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Abstract
The invention relates to the field of production of heating non-combustible cigarettes, in particular to a design method and application of a formula of a heating non-combustible cigarette leaf group. The method for designing the formula of the cigarette leaf group without burning by heating comprises the following steps: primarily selecting the tobacco raw material sprayed with the smoke agent through sensory quality evaluation under the heating condition; the primary selection of the tobacco raw materials is carried out by checking through a thermal analysis technology and a thermal cracking-gas chromatography-mass spectrometry combined technology; the check tobacco raw materials are subjected to a formula uniformity experiment through a material mixing uniformity experiment design, a mathematical model is established between sensory quality and the proportion of the raw material components, and an optimal formula is determined; preparing the cigarette without burning by heating according to the optimal leaf group formula, and carrying out sensory quality evaluation under the heating condition to verify the rationality of the optimal leaf group formula. The optimal leaf group formula of the cigarette which is not burnt during heating can be scientifically and reasonably designed, and the subjective experience defect is avoided.
Description
Technical Field
The invention relates to the field of production of heating non-combustible cigarettes, and in particular relates to a design method and application of a formula of a heating non-combustible cigarette leaf group.
Background
Different from the high-temperature combustion of the traditional cigarette, the cigarette without combustion is heated mainly by releasing the nicotine and the flavor components of the tobacco in a low-temperature heating mode, so that the chemical components released by cracking of the tobacco due to high-temperature combustion are reduced, the harmful components in the smoke of the cigarette are greatly reduced, and no sidestream smoke is released. The heating of the non-combustible cigarette has obvious advantages in the aspects of reducing environmental pollution and potential risks of smoking health, and is considered as the most development potential and most appropriate hotspot of future tobacco products by the international tobacco field.
Under the condition of low-temperature heating, the types and contents of aroma components released by tobacco raw materials used for heating the non-combustible cigarette are greatly different due to different types, production areas, parts, aroma types, years and the like, so that the sensory quality of the cigarette is different, and how to screen the tobacco raw materials and scientifically design a leaf composition formula becomes an important subject in the technical field of the formula of the non-combustible cigarette. At present, a unified and mature leaf group formula design technology is not available in the field of heating non-burning cigarettes, most formula designers can only select tobacco leaf raw materials according to a leaf group formula design method of a traditional cigarette by only depending on sensory evaluation, roughly design leaf group formulas by depending on subjective judgment and personal wishes, chemical bases and data support are lacked, and the defect of many artificial subjective factors exists.
Patents CN107897996A, CN107898001A and CN108030142A disclose a tobacco leaf raw material and its application in preparing cigarette which is not burned by heating, the tobacco leaf raw material group is prepared by mixing 6 kinds of raw materials, 8 kinds of raw materials and 9 kinds of raw materials, and pulverizing. The reconstituted tobacco is applied as a core material for preparing the cigarette which is not burnt by heating, the physical performance can better adapt to the processing requirement of forming equipment, the addition requirement of high-content smoke generating agent is met, the sensory quality meets the quality pursuit of the cigarette which is not burnt by heating, the aroma quality is better, the smoke concentration is higher, the texture is finer and smoother, the miscellaneous gas is slightly more, the stimulation is slightly more, the aftertaste is clean, and the harmony is better. Chinese patents ZL200810046379.4 and ZL200810046380.7 respectively disclose a cigarette leaf group formula design method and a selection method of substitute leaf groups in a cigarette formula, the method overcomes the defect that the prior art can not ensure that the sensory quality, the product style and the smoke index of tobacco leaf group formula meet the design requirements, and provides a method which can provide a plurality of formula combinations meeting the requirements, reduce the cost and reduce the workload of formula personnel. Patents ZL201510059244.1 and ZL201510058468.0 respectively disclose a method for designing a formula of a paper-making reconstituted tobacco raw material by separately extracting stem powder and mixing and extracting stem powder, and the raw material types are screened and determined by combining a chemical component quality sorting result and a sensory quality sorting result according to the design target requirements of products; and determining the mass ratio of the raw material types of the stem powder by using computer-aided design and sensory quality evaluation. The method overcomes the defect that in the prior art, a formula worker subjectively collocates various monomer raw materials according to experience and physically mixes the raw materials and then directly performs sensory evaluation to determine the leaf group formula, provides a leaf group formula uniform design method for preparing the paper-making reconstituted tobacco based on various monomer raw materials and then performing sensory evaluation, combines the expert experience and the modern computer technology, and provides a new idea for designing the paper-making reconstituted tobacco leaf group formula. Patent ZL200910116521.2 discloses a design method of a cigarette formula, which comprises dividing tobacco leaves in the formula into main material cigarettes, quasi-main material cigarettes and non-main material cigarettes; establishing a main material cigarette module consisting of all main material cigarettes, a secondary main material cigarette module consisting of all secondary main material cigarettes and a non-main material cigarette module consisting of all non-main material cigarettes; and performing mutual combination tests on the three modules to finally complete the formula design of the cigarette. Patent CN107568779A discloses a cigarette formula grouping design and processing method, which comprises two formulas, one is an auxiliary formula and the other is a basic formula.
The above tobacco leaf group formula design methods are all directed at traditional cigarettes or paper-making reconstituted tobaccos suitable for the traditional cigarettes, and the common characteristics of the tobacco leaf group formula design methods are that the tobacco leaf group formula design methods are suitable for high-temperature combustion conditions but not suitable for heating non-combustion cigarettes under low-temperature heating conditions. Most methods depend on the sensory evaluation conclusion of formula staff too much, lack the chemical substance basis and thermal analysis data support for screening the tobacco raw materials, and have the defects of more artificial subjective factors and the like.
The present application is made in view of this feature.
Disclosure of Invention
The invention aims to provide a method for designing a tobacco leaf composition formula of a heating non-burning cigarette, which can scientifically and reasonably design the optimal tobacco leaf composition formula of the heating non-burning cigarette and avoid the defect of subjective experience.
The invention also aims to provide the application of the formula design method of the heating non-combustible cigarette leaf group in the production of the tobacco sheets for the heating non-combustible cigarettes, and the application of the formula design method of the heating non-combustible cigarette leaf group in the production of the heating non-combustible cigarettes is realized, so that the prepared heating non-combustible cigarettes have more scientific and reasonable formula design of the leaf group, and the sensory quality of the heating non-combustible cigarettes is further improved.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a method for designing a formula of a cigarette leaf group which is not combusted by heating, which comprises the following steps:
carrying out sensory quality evaluation on the tobacco raw material sprayed with the smoke agent under the heating condition, and carrying out primary selection according to the sensory quality evaluation to obtain a primary selection tobacco raw material;
carrying out check on the primary selected tobacco raw material by utilizing a thermal analysis technology and a thermal cracking-gas chromatography-mass spectrometry combined technology to obtain a check tobacco raw material;
the check tobacco raw materials are subjected to formula uniformity experiments through the material mixing uniformity experiment design, a regression equation is established between the sensory quality evaluation score and the component proportion of the leaf group formula, variance analysis is carried out, and the optimal leaf group formula is determined;
preparing the cigarette without burning by heating according to the optimal leaf group formula, and carrying out sensory quality evaluation under the heating condition to verify the rationality of the optimal leaf group formula.
The invention provides an application of a formula design method of a heating non-combustion cigarette leaf group in the production of tobacco sheets for heating non-combustion cigarettes.
The embodiment of the invention provides a method for designing a formula of a cigarette leaf group without burning by heating, which has the beneficial effects that:
according to the method for designing the formula of the heating non-combustion cigarette leaf group, provided by the invention, through sensory quality evaluation under heating conditions, combination of a thermal analysis technology and a thermal cracking-gas chromatography combined technology and even material mixing experimental design, the subjective experience defect that in the prior art, a formulator simply utilizes sensory evaluation results under the traditional cigarette smoking conditions to design the formula of the heating non-combustion cigarette leaf group is overcome, and the formula design is more scientific, reasonable and practical.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a thermogravimetric plot provided by an embodiment of the present invention;
FIG. 2 is a differential thermogravimetric plot provided by an embodiment of the present invention;
fig. 3 is a total ion flow chromatogram provided by an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "first", "second", and the like are used only for distinguishing the description, and are not intended to indicate or imply relative importance.
The following specifically describes a design method of a formula of a cigarette leaf group without burning by heating and an application thereof provided by the embodiment of the invention.
The embodiment of the invention provides a method for designing a formula of a cigarette leaf group without burning by heating, which comprises the following steps:
s1, preparing materials and shredding;
various alternative tobacco raw materials are subjected to shredding treatment to prepare different types of cut tobaccos. The tobacco material can be selected from existing tobacco material types such as flue-cured tobacco, sun-cured red tobacco, sun-cured yellow tobacco, burley tobacco and aromatic tobacco.
S2, spraying a smoke agent;
and respectively spraying a smoke agent on the different types of tobacco shreds, and then baking and smoking the tobacco shreds. The smoke agent is used as an atomizing agent to generate aerosol, and volatile substances contained in the cut tobacco sprayed with the smoke agent form smoke under the auxiliary action of the smoke agent after the cut tobacco is heated.
Further, the smoke agent includes any one or a combination of plural kinds of polyhydric alcohols such as glycerin, 1, 2-propylene glycol, sorbitol, 1, 3-butylene glycol, esters of polyhydric alcohols, and polycarboxylic acid esters, and these plural kinds of substances can provide a good atomization effect.
Furthermore, the spraying amount of the smoke agent is 1% -20% of the mass of the tobacco raw materials, the proportion can achieve a good atomization effect, and the hair growth effect of smoke can be increased, so that the smoke is rich and full, and the smoking feeling is improved.
Preferably, the amount of the smoke agent sprayed is 5% to 15% by mass of the tobacco material, which ratio can further enhance the above effect.
S3, evaluating sensory quality, namely primarily selecting;
and evaluating sensory quality of the tobacco raw materials sprayed with the smoke agent under a low-temperature heating condition, grading according to the concentration of smoke, the strength and the amount of aroma, wherein the grading is divided into high grade, medium grade and low grade, and then selecting various tobacco shreds reaching high-grade evaluation as primary selection tobacco raw materials. The step can preliminarily screen out the tobacco shreds with strong smoke concentration, great strength and sufficient aroma amount as the primary selection tobacco raw materials for candidate.
Specifically, the cut tobacco with high concentration, high stiffness and sufficient aroma amount is high-grade, the cut tobacco with medium concentration, medium stiffness and medium aroma amount is medium-grade, and the cut tobacco with low concentration, low stiffness and flat aroma amount is low-grade.
Further, the heating temperature during the sensory quality evaluation is 300-.
It should be noted that the sensory quality evaluation criteria mainly refer to the national standard GB 5606.4-2005 cigarette part 4 sensory technical requirement, YC/T138 + 1998 tobacco and tobacco products sensory evaluation method, and YC/T498 + 2014 reconstituted tobacco (paper making method) sensory evaluation method.
S4, checking;
and carrying out check on the initially selected tobacco raw materials by utilizing a thermal analysis technology and a thermal cracking-gas chromatography-mass spectrometry combined technology to obtain the check tobacco raw materials. The step can further screen out high-quality tobacco shreds in the primarily selected tobacco raw materials, and then further determine the corresponding tobacco raw materials.
Specifically, a thermogravimetric curve, a differential thermogravimetric curve and a pyrolysis product gas chromatography total ion current chromatogram within the range of the pyrolysis temperature of 300-360 ℃ of each check tobacco raw material are obtained through a thermal analysis technology and a thermal cracking-gas chromatography-mass spectrometry technology. 300-360 ℃ is the working temperature range of the cigarette which is not burnt when being heated, and the total ion flow chromatogram of the pyrolysis product gas chromatogram in the temperature range has obvious scientificity and reference.
Thermogravimetric analysis refers to a thermal analysis technique for measuring the relationship between the mass and temperature change of a sample to be measured under programmed temperature control, and has become an effective tool for researching the combustion, pyrolysis process and dynamic behavior of biomass materials including tobacco. The thermogravimetric analysis process of the tobacco is highly similar to the low-temperature heating condition of heating non-combustible cigarettes, and the escaping gas product in the thermal weight loss process directly forms the aerosol component in the smoke. The residue percentage at a specific temperature can be obtained from the thermogravimetric curve, the escaping gas percentage can be further obtained, and the weight loss rate values corresponding to the maximum weight loss rates at different pyrolysis stages can be obtained from the differential thermogravimetric curve.
It should be noted that the thermal analysis technique includes any one or more combinations of a single thermogravimetric analysis and a thermogravimetric analyzer or a simultaneous thermogravimetric analyzer in combination with various other analytical instruments, such as a thermogravimetric analysis-infrared (TG/STA-FTIR), a thermogravimetric analysis-gas mass spectrometry (TG/STA-GC-MS), a thermogravimetric analysis-mass spectrometry (TG/STA-MS), and a simultaneous thermogravimetric analysis-infrared-gas mass spectrometry (STA-FTIR-GC/MS).
Further, obtaining a maximum weight loss rate value of the primary selected tobacco raw materials according to a differential thermogravimetric curve, and sequencing the primary selected tobacco raw materials according to the maximum weight loss rate value, so as to determine the primary selected tobacco raw materials with a higher maximum weight loss rate value, wherein a higher weight loss rate value means a faster release rate of aroma components in the cut tobacco, that is, a faster pyrolysis volatilization speed of the cut tobacco at the same external heating temperature, and the more aroma components the consumer can catch in a 2-3 second smoking time, the better satisfaction.
The weight loss rate values comprise two weight loss rate values corresponding to a second pyrolysis stage and a third pyrolysis stage, wherein the second pyrolysis stage mainly refers to the precipitation of endogenous volatile components of the cut tobacco and is accompanied with the thermal decomposition of cut tobacco components; the third pyrolysis stage mainly means aerobic cracking of tobacco biopolymers accompanied by further transfer of endogenous chemical components, and two weight loss rate values corresponding to the second pyrolysis stage and the third pyrolysis stage can represent volatilization speeds of volatile substances in tobacco shreds, so that the two sorting steps need to be considered simultaneously.
Further, according to the thermogravimetric curve and the differential thermogravimetric curve, the residue rate difference of the primary selection tobacco raw materials in the heating temperature range of 200-400 ℃ is obtained, the primary selection tobacco raw materials are sequenced according to the residue rate difference, and therefore the primary selection tobacco raw materials with the larger residue rate difference are determined, the temperature range of 200-400 ℃ is the corresponding temperature range when the weight loss rate of the tobacco shreds is higher, the residue rate difference is the proportion of escaping gas, the higher the proportion is, the higher the release amount of the flavor components in the tobacco shreds is, the more favorable the sensory quality is, therefore, the primary selection tobacco raw materials with the larger residue rate difference in the heating temperature range of 200-400 ℃ can be selected, the release amount and the release speed of the flavor components in the tobacco shreds can be considered at the same time, and the higher quality tobacco shreds are further screened.
Preferably, the heating temperature is 200-. The temperature range can further give consideration to the release amount and release speed of the flavor components in the tobacco shreds.
On the other hand, the single thermal analysis technology cannot determine the type and content of volatile pyrolysis products, and the thermal cracking-gas chromatography-mass spectrometry technology has an aerobic cracking process which is highly similar to the smoking moment of heating non-combustible cigarettes at a specific thermal cracking temperature, so that the thermal cracking-gas chromatography-mass spectrometry technology can be used for directly representing the pyrolysis products of tobacco shreds under a heating condition, and the pyrolysis products form a chemical substance basis of sensory quality. The total ion current chromatogram and the mass spectrogram of the cracked product at a certain cracking temperature can be obtained by the thermal cracking-gas chromatography-mass spectrometry technology, and the possible structures of the product components can be determined by searching in an NIST (nickel-in-sequence analysis) spectrogram database and the relative content can be calculated according to the peak area, so that support is provided for screening the tobacco raw materials from the types and the content of the aroma components.
Further, the types and the contents of pyrolysis components of the primary selected tobacco raw materials are obtained according to the pyrolysis product gas chromatography total ion current chromatogram and the mass spectrum library retrieval result, and the primary selected tobacco raw materials with more types and higher contents of the pyrolysis components are determined according to the types and the contents, wherein the more types of the pyrolysis components indicate that the richness of aroma in smoke is higher, the higher content of the pyrolysis components indicates that the amount of aroma components is higher, and the two points also represent important embodying standards for sensory quality of the non-combustible heated cigarette.
It should be noted that, the types of pyrolysis components are referred to first, and then the contents of the components are referred to on the basis of the larger types.
Further, screening and evaluating analysis results of the comprehensive thermogravimetric curve, the differential thermogravimetric curve and the pyrolysis product gas chromatography total ion current chromatogram, and selecting the primary selection tobacco raw material with larger residue rate difference, higher weight loss rate value, more pyrolysis component types and higher content as the check tobacco raw material. The three components are integrated to obtain the high-quality tobacco raw material which simultaneously gives consideration to the release amount and release speed of the flavor components and the more complex and diversified flavor components with layering feeling.
The difference of the residue rates is larger than or equal to 35%, the weight loss rate value is higher than 50% -60% before the weight loss rate value is sorted, the types of the pyrolysis components are more than or equal to 30, the relative contents refer to nicotine, aldehydes, olefins, ketones, furanones, pyrones, phenols, nitrogen heterocycles, alcohol, acid and esters, and the tobacco raw materials with the contents of nicotine, aldehydes, olefins, ketones, pyrones, phenols, nitrogen heterocycles of more than or equal to 40%, aldehydes of more than or equal to 10%, olefins of more than or equal to 5%, ketones of more than or equal to 5%, furanones, pyrones of more than or equal to 2%, phenols of more than or equal to 2%, and alcohol, acid and esters of more than or equal to 2% are selected as the tobacco raw materials.
S5, designing a leaf group formula;
aiming at the multiple selected check tobacco raw materials, multiple leaf group formulas are obtained through a uniform mixing experimental design. The specific processes, methods and calculations can be referred to in design of homogeneous mixing experiments (Ningjianghui, university of Master in China, doctor's academic thesis, 2008) and DPS data processing System (Ching-Tang, science publishers, second edition, 2010).
S6, determining an optimal leaf group formula;
preparing multiple cigarettes which are not combusted by heating according to the multiple leaf group formulas by the same preparation method, respectively carrying out sensory quality evaluation after heating, establishing a regression equation between the sensory quality evaluation score and the component proportion of the leaf group formulas, analyzing, and determining the optimal leaf group formula.
It should be noted that the analysis method of the regression equation includes a visual analysis method and a regression analysis method.
S7, verifying the optimal leaf group formula;
preparing the cigarette without burning by heating according to the optimal leaf group formula, and carrying out sensory quality evaluation under the heating condition to verify the rationality of the optimal leaf group formula.
The preparation method of the tobacco sheet for cigarette by heating and non-combustion comprises any one or more of rolling method, thick paste method, dry method and modified rolling method, thick paste method and dry method. The tobacco sheet is prepared by the method, and then the prepared tobacco sheet is used for preparing the cigarette which is not combusted by heating.
The embodiment of the invention also provides application of the formula design method of the tobacco leaf group for the heating non-combustion cigarette in production of tobacco sheets for the heating non-combustion cigarette.
Specifically, according to production requirements, an optimal leaf group formula is designed according to any one of the above methods for designing a leaf group formula of a heating non-combustible cigarette, then tobacco sheets are prepared according to the optimal leaf group formula by different preparation methods, and then the heating non-combustible cigarette is prepared by using the prepared different tobacco sheets. Thereby realizing the application of the method for designing the formula of the tobacco leaf group for the heating non-combustion cigarette in the production of tobacco sheets for the heating non-combustion cigarette.
The features and properties of the present invention are described in further detail below with reference to examples.
The embodiment provides a method for designing a formula of a cigarette leaf group without burning by heating, which comprises the following steps:
firstly, selecting 12 fresh-scent, middle-scent and strong-scent tobacco raw materials, shredding, spraying a smoke agent, drying tobacco shreds and striking tobacco shreds, wherein the shredding width is 1 mm, the smoke agent is selected from glycerin, the spraying amount is 10% of the mass of the tobacco shreds, the temperature of the tobacco shreds drying is 80 ℃, then carrying out sensory quality evaluation under the heating condition of 350 ℃, selecting high-grade tobacco shreds, namely the tobacco shreds with strong concentration, strong strength and sufficient aroma amount, and obtaining 8 primary-selected tobacco raw materials, which are marked as A, B, C, D, E, F, G and H.
And performing thermogravimetric analysis on the 8 primary selected tobacco raw materials by using a thermal analysis technology to obtain a thermogravimetric curve and a differential thermogravimetric curve, wherein the specific results are respectively shown in the figure 1 and the figure 2. Selecting 350 ℃ as the thermal cracking temperature, enabling the pyrolysis product to enter a gas chromatograph-mass spectrometer on line to obtain a corresponding total ion current chromatogram, and obtaining a specific result as shown in figure 3.
Obtaining a thermogravimetric analysis data table according to the thermogravimetric curve and the thermogravimetric differential curve, referring to table 1, then selecting a primary selection tobacco raw material with the residue rate difference of more than or equal to 35% in the heating temperature range of 200 ℃ and 400 ℃, and respectively marking the residue rates corresponding to 200 ℃ and 350 ℃ as M200、M350If it is not, it is leftThe difference of the slag rate is recorded as M200-M350As can be seen from table 1, the difference Δ M between the residue rates was A, B, C, D, E, F, G and H in the order from high to low.
According to a differential thermogravimetric curve, the maximum weight loss rate of the 8 tobacco shreds in the second pyrolysis stage is compared and is marked as V2H, F, G, D, E, C, A and B are shown in sequence from high to low. Similarly, the maximum weight loss rate of 8 tobacco shreds in the third pyrolysis stage is compared and is marked as V3C, B, A, D, H, F, E and G are shown in sequence from high to low.
Obtaining the types and the contents of thermal cracking products of different tobacco raw materials at 350 ℃ according to the total ion current chromatogram and the mass spectrum library retrieval and analysis, and comprehensively comparing delta M, V1、V2And the results of the analysis of the kind and content of the pyrolysis product, 5 cut tobaccos were obtained as the check tobacco materials, which were designated A, B, C, D and E, respectively.
TABLE 1 thermogravimetric analysis data Table
| Raw material numbering | M200(％) | M350(％) | ΔM(％) | V2(％/min) | V3(％/min) |
| A | 88.97 | 47.76 | 41.2 | 4.29 | 7.5 |
| B | 87.46 | 48.85 | 38.6 | 4.24 | 7.5 |
| C | 83.00 | 45.86 | 37.1 | 4.53 | 8.0 |
| D | 85.07 | 49.32 | 35.8 | 4.96 | 6.7 |
| E | 84.47 | 49.37 | 35.1 | 4.8 | 6.3 |
| F | 89.15 | 54.74 | 34.4 | 5.61 | 6.5 |
| G | 91.99 | 62.66 | 29.3 | 5.12 | 6.1 |
| H | 86.05 | 61.27 | 24.8 | 5.63 | 6.6 |
Then, 5 kinds of check tobacco raw materials are subjected to formula uniform design, the raw material inventory, the raw material cost and the characteristic difference of different raw materials are considered, a mixing formula design with upper and lower limit constraints is adopted, and the upper and lower limits are set according to a table 2. Selection of 5-factor 10 level design recipe experiment UM based on DPS data processing System (V14.10)10(105) And obtaining a mixed material uniform experimental design scheme with upper and lower limit constraints, and referring to a table 3. The method comprises the steps of preparing tobacco raw material components into tobacco sheets for heating non-combustion cigarettes according to a dry preparation process by using the limited mixed material uniform design scheme, preparing the tobacco sheets into the heating non-combustion cigarettes, carrying out sensory quality evaluation under the heating condition, setting the sensory quality score as Y and the component proportions as X1, X2 and X3 … X5, establishing a regression equation between Y and X1, X2 and X3 … X5 through quadratic polynomial stepwise regression, and determining an optimal formula which accords with the sensory quality by using an intuitive analysis method and a regression analysis method.
TABLE 2 design scheme of material mixing uniformity experiment with upper and lower limit constraints
| Upper and lower limits adjusted by each factor | ||||||
| Factor(s) | Lower limit of | Upper limit of | ||||
| X1 | 0.3 | 0.4 | ||||
| X2 | 0.2 | 0.3 | ||||
| X3 | 0.1 | 0.2 | ||||
| X4 | 0.05 | 0.1 | ||||
| X5 | 0.05 | 0.1 | ||||
| Design scheme of mixing test | ||||||
| Coefficient of centrifugation, α is 0.50 |
Table 3 mixing uniformity experimental design data
According to table 3, the visual analysis method shows that when X1 is 0.3914, X2 is 0.2565, X3 is 0.1938, X4 is 0.0638, and X5 is 0.0946, the sensory quality score has a maximum value Y of 88.
And (3) carrying out quadratic polynomial stepwise regression on the experimental data by using DPS data processing software to obtain a regression equation between the sensory quality Y and each component Xi as follows:
Y＝307.0073555-4180.645330*X1+7383.627042*X3-2810.8970314*X4 +3107.9430345*X3*X3+14886.474618*X4*X4+14408.938389*X1*X2 -29514.487309*X2*X3+724.1939183*X3*X4。
the corresponding complex correlation coefficient R is 0.9999, the decision coefficient R2 is 0.9999, and the analysis of variance shows that p is 0.0316 < 0.05, indicating that the relationship between the variables of the regression equation is significant. See table 4 for specific results.
TABLE 4 ANOVA TABLE
| Source of variation | Sum of squares | Degree of freedom | Mean square | F value | p value |
| Regression | 250.3479 | 8 | 31.29349 | 600.5082 | 0.031551 |
| Residual error | 0.052112 | 1 | 0.052112 | ||
| Total variation | 250.4 | 9 |
Planning and solving the regression equation, and when X1 is 0.3378, X2 is 0.2417, X3 is 0.1938, X4 is 0.0610 and X5 is 0.1657, obtaining the maximum value Y of the sensory quality Y of the regression equation 128.8149, integrating a visual analysis method and a regression analysis method, and selecting a regression analysis result as an optimization scheme: that is, when X1 is 0.34, X2 is 0.24, X3 is 0.19, X4 is 0.06, and X5 is 0.17, the formula is the optimal leaf group formula.
According to the optimal leaf group formula, the tobacco sheets are prepared according to a dry preparation process, the tobacco sheets are prepared into the cigarette which is not combusted under heating, sensory quality evaluation is carried out under the heating condition, the rationality of the optimal formula is verified, the sensory quality of the cigarette which is not combusted under heating and is produced according to the optimal formula is proved to be 89, and the reasonable design of the leaf group formula obtained through optimization is proved.
The embodiment also provides application of the formula design method of the tobacco leaf group for the heating non-combustion cigarette in the production of tobacco sheets for the heating non-combustion cigarette.
Specifically, according to production requirements, an optimal leaf group formula is designed according to any one of the above methods for designing a leaf group formula of a heating non-combustible cigarette, then tobacco sheets are prepared according to the optimal leaf group formula by different preparation methods, and then the heating non-combustible cigarette is prepared by using the prepared different tobacco sheets. Thereby realizing the application of the method for designing the formula of the tobacco leaf group for the heating non-combustion cigarette in the production of tobacco sheets for the heating non-combustion cigarette.
In conclusion, the method for designing the formula of the heating non-combustion cigarette leaf group overcomes the subjective experience defect that a formulator simply utilizes the sensory evaluation result under the traditional cigarette smoking condition to design the formula of the heating non-combustion cigarette leaf group in the prior art through sensory quality evaluation, a thermal analysis technology, a thermal cracking-gas chromatography-mass spectrometry combined technology and a mixed material uniformity experimental design under the heating condition, and enables the formula design to be more scientific, reasonable and practical.
The embodiment of the invention also provides application of the formula design method of the tobacco leaf group for the heating non-combustion cigarette in the production of tobacco sheets for the heating non-combustion cigarette. The application of the method for designing the tobacco leaf composition formula of the heating non-combustion cigarettes in the production of the heating non-combustion cigarettes is realized, so that the prepared heating non-combustion cigarettes have more scientific and reasonable tobacco leaf composition formula design, and the sensory quality of the heating non-combustion cigarettes is further improved.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (9)
1. A method for designing a formula of a cigarette leaf group which is not combusted by heating is characterized by comprising the following steps:
carrying out sensory quality evaluation on the tobacco raw material sprayed with the smoke agent under the heating condition, and carrying out primary selection according to the sensory quality evaluation result to obtain a primary selection tobacco raw material;
carrying out check on the primary selected tobacco raw material by utilizing a thermal analysis technology and a thermal cracking-gas chromatography-mass spectrometry combined technology to obtain a check tobacco raw material;
the check tobacco raw materials are subjected to a formula uniformity experiment through a material mixing uniformity experiment design, a regression equation is established between sensory quality evaluation scores and component proportions of the formula uniformity experiment, variance analysis is carried out, and an optimal leaf group formula is determined;
preparing a cigarette which is not combusted by heating according to the optimal leaf group formula, and evaluating sensory quality under heating conditions to verify the rationality of the optimal leaf group formula;
the sensory quality evaluation is carried out under the low-temperature heating condition, and the temperature range of the low-temperature heating is 300-360 ℃;
obtaining a thermogravimetric curve, a differential thermogravimetric curve and a total ion flow chromatogram of the pyrolysis product gas chromatogram within the range of the thermal cracking temperature of 300-;
obtaining the residue rate difference of the primary selection tobacco raw materials within the range of heating temperature of 200-;
and (3) integrating the thermogravimetric curve, the differential thermogravimetric curve and the analysis result of the total ion current chromatogram of the pyrolysis product gas chromatography, and selecting the primary selection tobacco raw material with larger residue rate difference, higher weight loss rate value, more pyrolysis component types and higher content as the check tobacco raw material.
2. The method for designing the formula of the tobacco leaf set for the non-burning cigarettes according to claim 1, wherein the sensory quality evaluation is to conduct sensory evaluation on the non-burning cigarettes under the condition of low-temperature heating, and the evaluation is carried out according to the smoke concentration, the strength and the aroma amount, wherein the evaluation is divided into three grades, namely high grade, medium grade and low grade, wherein the grade with high concentration, high strength and sufficient aroma amount is high grade, the grade with medium concentration, medium strength and medium aroma amount is medium grade, and the grade with low concentration, low strength and flat aroma amount is low grade.
3. The method for designing a tobacco composition formula for a non-combustible heated cigarette as claimed in claim 1, wherein the difference between the residue rates of the primary selected tobacco raw materials within the range of heating temperature of 200-350 ℃ is obtained according to the thermogravimetric curve and the differential thermogravimetric curve, and the primary selected tobacco raw materials are sorted according to the difference between the residue rates.
4. The method of claim 1, wherein the thermal analysis technique comprises any one or more of a single thermogravimetric analysis and a combination of a thermogravimetric analyzer or a simultaneous thermal analyzer with various other analytical instruments.
5. The method for designing a tobacco leaf composition formulation capable of being burned under heating according to claim 1, wherein the amount of the smoke agent sprayed is 1 to 20% by mass of the tobacco raw material.
6. The method for designing a tobacco leaf composition formula without burning by heating according to claim 1, wherein the amount of the smoke agent sprayed is 5 to 15% by mass of the tobacco raw material.
7. The method for designing a tobacco leaf set formulation for a heat non-combustible cigarette according to claim 1, wherein the method for preparing the tobacco sheet for a heat non-combustible cigarette comprises any one or a combination of a rolling method, a thick pulp method and a dry method.
8. The method of claim 1, wherein the smoking agent comprises any one or more of glycerol, 1, 2-propanediol, sorbitol, 1, 3-butanediol, esters of polyhydric alcohols, and esters of polycarboxylic acids.
9. Use of the method of claim 1 in the manufacture of tobacco sheet for a heat non-combustible cigarette.
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